WO2018201650A1 - 用于外墙保温层的建筑材料制备方法及其应用 - Google Patents

用于外墙保温层的建筑材料制备方法及其应用 Download PDF

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WO2018201650A1
WO2018201650A1 PCT/CN2017/100478 CN2017100478W WO2018201650A1 WO 2018201650 A1 WO2018201650 A1 WO 2018201650A1 CN 2017100478 W CN2017100478 W CN 2017100478W WO 2018201650 A1 WO2018201650 A1 WO 2018201650A1
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parts
building material
insulation layer
reaction product
hot pressing
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PCT/CN2017/100478
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French (fr)
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屠志豪
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苏州轩朗塑料制品有限公司
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/91Polymers modified by chemical after-treatment
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/325Calcium, strontium or barium phosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Definitions

  • the invention relates to the technical field of building materials, in particular to a method for preparing building materials for an outer wall insulation layer and an application thereof.
  • the annual housing area is as high as 1.6 billion to 2 billion square meters, and about 95% is high-energy buildings. At present, the ratio of building energy consumption to total national energy consumption is about 30%.
  • Energy shortage has become the soft underbelly of China's economic development.
  • External wall insulation is a kind of building insulation energy-saving technology that is currently being promoted.
  • the external thermal insulation Compared with the internal thermal insulation, the external thermal insulation has reasonable technical advantages and has obvious advantages.
  • the thermal insulation material with the same specifications, the same size and performance has better external heat preservation effect than the internal thermal insulation.
  • the external thermal insulation technology is not only suitable for new buildings, but also for the renovation of old buildings. It is suitable for a wide range; the external thermal insulation package is on the outer side of the main structure, which can protect the main structure and prolong the life of the building; effectively reduce the thermal bridge of the building structure. It does not affect the original effective space of the building; it also eliminates condensation and improves the comfort of living.
  • the present invention provides a method for preparing a building material for an outer wall insulation layer, which is obtained by wet-ball milling quartz sand, kaolin clay and talc powder, and then calcined by powdering. Further, a modified carboxylated polyester resin and a mixture of sonicated acetyl tributyl citrate, hexamethylenetetramine and strontium phosphate are added together to carry out a heating reaction, followed by kneading, vulcanization, hot pressing, and the like. The specific process is used to make finished building materials. The prepared building materials have good flame retarding effect, weather resistance and aging resistance, and have good application prospects. At the same time, the application of the building material for the outer wall insulation layer prepared by the preparation method in the building wall material is also disclosed.
  • the method for preparing building materials for exterior wall insulation consists of the following steps:
  • the mixed slurry obtained in the step (1) is dried into a powder, and then added to a calcining furnace, calcined at 1000-1200 ° C for 50 min, and then rapidly cooled to room temperature to obtain a calcined product;
  • the intermediate reaction product of the step (6) is vulcanized at 150 ° C for 45 min, and cooled to room temperature to obtain a sulfurized reactant;
  • the sulfurized reactant obtained in the step (7) is pulverized into pellets, and sufficiently mixed with 2-4 parts of the crosslinking agent to obtain a mixed material, and then the mixture is placed in a preformed molding die for heat.
  • the pressure, the hot pressing temperature is 100-120 ° C, the hot pressing time is 4-5 h, and after the hot pressing is completed, it is cooled to room temperature to obtain a finished material.
  • the ball mill ratio of the ball mill in the step (1) is 15:1.
  • the degree of vacuum in the step (2) is preferably -0.08 MPa.
  • the crosslinking agent in the step (8) is selected from any one of isooctyl acrylate, glycerin dimethacrylate, and triethanolamine.
  • the invention also provides the application of the building material for the outer wall insulation layer obtained by the above preparation method in the building wall material.
  • the invention has the following beneficial effects:
  • the method for preparing a building material for an outer wall insulation layer of the present invention is carried out by wet ball milling of quartz sand, kaolin, talc powder, drying into powder, calcination, addition of modified carboxyl polyester resin, and sonication.
  • the mixture of acetyl tributyl citrate, hexamethylenetetramine and strontium phosphate is subjected to a heating reaction, followed by a series of specific processes such as kneading, vulcanization and hot pressing to produce a finished building material.
  • the prepared building materials have good flame retarding effect, weather resistance and aging resistance, and have good application prospects.
  • the present invention makes a significant mention of the material properties of the final prepared building materials by modifying the carboxyl polyester resin by a specific process, compared to the addition of only the unmodified carboxyl polyester resin. In fact, unexpected technical effects have been achieved.
  • the method for preparing a building material for an exterior wall insulation layer of the present invention is inexpensive, has a simple method, is suitable for large-scale industrial use, and has high practicability.
  • the mixed slurry obtained in the step (1) is dried into a powder, then added to a calciner, calcined at 1000 ° C for 50 min, and then rapidly cooled to room temperature to obtain a calcined product;
  • the intermediate reaction product of the step (6) is vulcanized at 150 ° C for 45 min, and cooled to room temperature to obtain a sulfurized reactant;
  • the sulfurized reactant obtained in the step (7) is pulverized into pellets, and sufficiently mixed with 2 parts of isooctyl acrylate to obtain a mixture, and then the mixture is placed in a preformed molding die for hot pressing.
  • the hot pressing temperature is 100 ° C
  • the hot pressing time is 4 h
  • the mixed slurry obtained in the step (1) is dried into a powder, and then added to a calcining furnace, calcined at 1100 ° C for 50 min, and then rapidly cooled to room temperature to obtain a calcined product;
  • the intermediate reaction product of the step (6) is vulcanized at 150 ° C for 45 min, and cooled to room temperature to obtain a sulfurized reactant;
  • the sulfurized reactant obtained in the step (7) is pulverized into pellets, and fully mixed with 3 parts of glycerin dimethacrylate to obtain a mixture, and then the mixture is placed in a preformed molding die.
  • the hot pressing, the hot pressing temperature is 110 ° C, the hot pressing time is 4.5 h, and after the hot pressing is completed, it is cooled to room temperature to obtain a finished material.
  • the mixed slurry obtained in the step (1) is dried into a powder, and then added to a calcining furnace, calcined at 1200 ° C for 50 min, and then rapidly cooled to room temperature to obtain a calcined product;
  • the intermediate reaction product of the step (6) is vulcanized at 150 ° C for 45 min, and cooled to room temperature to obtain a sulfurized reactant;
  • the sulfurized reaction product obtained in the step (7) is pulverized into pellets, and fully mixed with 4 parts of triethanolamine to obtain a mixed material, and then the mixture is placed in a preformed molding die for hot pressing, heat.
  • the pressing temperature was 120 ° C
  • the hot pressing time was 5 h
  • the mixed slurry obtained in the step (1) is dried into a powder, and then added to a calciner, calcined at 800 ° C for 50 min, and then rapidly cooled to room temperature to obtain a calcined product;
  • the intermediate reaction product of the step (6) is vulcanized at 180 ° C for 45 min, and cooled to room temperature to obtain a sulfurized reactant;
  • the sulfurized reactant obtained in the step (7) is pulverized into pellets, and sufficiently mixed with 2 parts of isooctyl acrylate to obtain a mixture, and then the mixture is placed in a preformed molding die for hot pressing.
  • the hot pressing temperature is 100 ° C
  • the hot pressing time is 4 h
  • the sulfurized reaction product obtained in the step (6) is pulverized into pellets, and mechanically mixed with 3 parts of glycerin dimethacrylate to obtain a mixture, and then the mixture is placed in a preformed molding die.
  • the hot pressing, the hot pressing temperature is 110 ° C, the hot pressing time is 4.5 h, and after the hot pressing is completed, it is cooled to room temperature to obtain a finished material.
  • ultrasonic treatment (3) 15 parts of acetyl tributyl citrate, 9 parts of hexamethylenetetramine, and 3 parts of cesium phosphate were mixed, and 2000 mL of deionized water was added for ultrasonic treatment.
  • the conditions of ultrasonic treatment were: temperature 60. °C, ultrasonic power 800W, ultrasonic time 35min; obtained ultrasonic treatment mixture;
  • the mixed slurry obtained in the step (1) is dried into a powder, and then added to a calcining furnace, calcined at 1200 ° C for 50 min, and then rapidly cooled to room temperature to obtain a calcined product;
  • the preliminary reaction product of the step (5) is vulcanized at 150 ° C for 45 min, and cooled to room temperature to obtain a sulfurized reactant;
  • the sulfurized reactant obtained in the step (6) is pulverized into pellets, and fully mixed with 4 parts of triethanolamine to obtain a mixed material, and then the mixture is placed in a preformed molding die for hot pressing, heat.
  • the pressing temperature was 120 ° C
  • the hot pressing time was 5 h
  • Example 1-3 The building materials prepared in Examples 1-3 and Comparative Examples 1-3 were subjected to three tests of combustion performance grade, impermeability grade, and linear shrinkage ratio, and the test results are shown in Table 1.
  • the method for preparing building materials for exterior wall insulation layer of the present invention comprises quartz sand, kaolin, The talc is wet-ball milled, dried and then calcined, and then a modified carboxylated polyester resin and a mixture of sonicated acetyl tributyl citrate, hexamethylenetetramine and strontium phosphate are used for heating reaction.
  • the finished building materials are then processed through a series of specific processes such as mixing, vulcanization and hot pressing.
  • the prepared building materials have good flame retarding effect, weather resistance and aging resistance, and have good application prospects.
  • the preparation method of the building material for the outer wall insulation layer of the invention has the advantages of low cost raw materials, simple method, large-scale industrial application, and strong practicability.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
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Abstract

一种用于外墙保温层的建筑材料制备方法及其应用,该方法通过将石英砂、高岭土、滑石粉湿法球磨,干燥成粉后煅烧,再加入经改性的羧基聚酯树脂以及经超声处理的乙酰柠檬酸三丁酯、六次甲基四胺和磷酸钡的混合物共同进行加热反应,随后经混炼、硫化、热压等一系列特定工艺制成成品建筑材料。制备而成的建筑材料,其阻燃效果好,耐候、耐老化,具有较好的应用前景。同时还涉及由该制备方法制得的建筑材料在建筑墙体材料中的应用。

Description

用于外墙保温层的建筑材料制备方法及其应用 技术领域
本发明涉及建筑材料这一技术领域,特别涉及到用于外墙保温层的建筑材料制备方法及其应用。
背景技术
我国能源短缺,特别是目前又正处于建设鼎盛期,每年建成的房屋面积高达16亿至20亿平方米,而约95%以上是高能耗建筑。目前,建筑能耗占全国总能耗的比例约为30%。能源短缺已成为我国经济发展的软肋。外墙保温是目前大力推广的一种建筑保温节能技术。
外保温与内保温相比,技术合理,有其明显的优越性,使用同样规格、同样尺寸和性能的保温材料,外保温比内保温的效果好。外保温技术不仅适用于新建建筑,也适用于旧楼改造,适用于范围广;外保温包在主体结构的外侧,能够保护主体结构,延长建筑物的寿命;有效减少了建筑结构的热桥,不影响建筑的原有有效空间;同时消除了冷凝,提高了居住的舒适度。目前应用较多的外墙保温技术主要有:外挂式外保温、聚苯板与墙体一次浇注成型、聚苯颗粒保温浆料外墙保温等,均取得了较好的效果。由于有机保温材料导热系数低,隔热保温性能良好,目前被广泛应用于外墙保温。但是有机保温材料存在着种种弊端,比如原材料使用石油资源、环保性差、易燃、耐候性差、易老化等。尤其是随着推广应用进一步深入,有机保温材料易燃的缺陷逐步暴露,严重的威胁到人们的安全。
发明内容
为解决上述技术问题,本发明提供用于外墙保温层的建筑材料制备方法,该方法通过将石英沙、高岭土、滑石粉湿法球磨,干燥成粉后煅烧, 再加入经改性的羧基聚酯树脂以及经超声处理的乙酰柠檬酸三丁酯、六次甲基四胺和磷酸钡的混合物共同进行加热反应,随后经混炼、硫化、热压等一系列特定工艺制成成品建筑材料。制备而成的建筑材料,其阻燃效果好,耐候、耐老化,具有较好的应用前景。同时还公开了由该制备方法制得的用于外墙保温层的建筑材料在建筑墙体材料中的应用。
本发明的目的可以通过以下技术方案实现:
用于外墙保温层的建筑材料制备方法,由以下步骤组成:
(1)将石英沙20-25份、高岭土15-20份、滑石粉8-12份混合均匀置于球磨机中,经湿法球磨,得到粒度150-180目的混合料浆;
(2)将羧基聚酯树脂22-28份置于反应釜中,升温至150℃,在真空条件下处理2-3h,随后升温至175℃,加入四丁酚醛6-10份、聚己二酸乙二醇酯3-5份、甲氧基聚乙二醇2-4份,在常压下反应1h,将反应产物用3mol/L的稀盐酸洗涤2-3次,然后用去离子水洗涤至中性,得改性羧基聚酯树脂;
(3)将乙酰柠檬酸三丁酯6-15份、六次甲基四胺3-9份、磷酸钡1-3份混合,加入2000mL去离子水,进行超声处理,超声处理的条件为:温度50-60℃,超声功率800W,超声时间25-35min;得超声处理混合物;
(4)将步骤(1)得到的混合料浆干燥成粉,随后加入煅烧炉中,在1000-1200℃下,煅烧50min,然后迅速降温至室温,得煅烧产物;
(5)将步骤(4)的煅烧产物加入反应釜中,加热反应釜,待温度达到115℃时,再向反应釜中加入步骤(2)所得的改性羧基聚酯树脂和步骤(3)所得的超声处理混合物,混合均匀后保温反应30min,得初步反应产物;
(6)将步骤(5)所得的初步反应产物倒入混炼机中,调节混炼机温度至130-150℃,随后向混炼机中加入氯化石蜡3-5份,在120-150rpm的 搅拌速率下混炼15-20min,得中间反应产物;
(7)将步骤(6)的中间反应产物在150℃的条件下硫化45min,冷却至室温后得硫化反应物;
(8)将步骤(7)得到的硫化反应物粉碎成颗粒状,与交联剂2-4份进行充分机械混匀并得到混合物料,随后将上述混合物料放置在预制的成型模具内进行热压,热压温度为100-120℃,热压时间为4-5h,热压完成后冷却至室温,得到成品材料。
优选地,所述步骤(1)中球磨机的球料比为15:1。
优选地,所述步骤(2)中的真空度优选为-0.08Mpa。
优选地,所述步骤(8)中的交联剂选自丙烯酸异辛酯、甘油二甲基丙烯酸酯、三乙醇胺中的任意一种。
本发明还提供了由上述制备方法得到的用于外墙保温层的建筑材料在建筑墙体材料中的应用。
本发明与现有技术相比,其有益效果为:
(1)本发明的用于外墙保温层的建筑材料制备方法通过将石英沙、高岭土、滑石粉湿法球磨,干燥成粉后煅烧,再加入经改性的羧基聚酯树脂以及经超声处理的乙酰柠檬酸三丁酯、六次甲基四胺和磷酸钡的混合物共同进行加热反应,随后经混炼、硫化、热压等一系列特定工艺制成成品建筑材料。制备而成的建筑材料,其阻燃效果好,耐候、耐老化,具有较好的应用前景。
(2)本发明通过将羧基聚酯树脂经特定工艺进行改性,使得最后所制备得到的建筑材料在材料性能上有了显著提到,相比较于只添加未经改性的羧基聚酯树脂而言,取得了预料不到的技术效果。
(3)本发明的用于外墙保温层的建筑材料的制备方法所用原料廉价、方法简单,适于大规模工业化运用,实用性强。
具体实施方式
下面结合具体实施例对发明的技术方案进行详细说明。
实施例1
(1)将石英沙20份、高岭土15份、滑石粉8份混合均匀置于球磨机中,经湿法球磨,得到粒度150目的混合料浆;
(2)将羧基聚酯树脂22份置于反应釜中,升温至150℃,在真空度为-0.08Mpa的条件下处理2h,随后升温至175℃,加入四丁酚醛6份、聚己二酸乙二醇酯3份、甲氧基聚乙二醇2份,在常压下反应1h,将反应产物用3mol/L的稀盐酸洗涤2-3次,然后用去离子水洗涤至中性,得改性羧基聚酯树脂;
(3)将乙酰柠檬酸三丁酯6份、六次甲基四胺3份、磷酸钡1份混合,加入2000mL去离子水,进行超声处理,超声处理的条件为:温度50℃,超声功率800W,超声时间25min;得超声处理混合物;
(4)将步骤(1)得到的混合料浆干燥成粉,随后加入煅烧炉中,在1000℃下,煅烧50min,然后迅速降温至室温,得煅烧产物;
(5)将步骤(4)的煅烧产物加入反应釜中,加热反应釜,待温度达到115℃时,再向反应釜中加入步骤(2)所得的改性羧基聚酯树脂和步骤(3)所得的超声处理混合物,混合均匀后保温反应30min,得初步反应产物;
(6)将步骤(5)所得的初步反应产物倒入混炼机中,调节混炼机温度至130℃,随后向混炼机中加入氯化石蜡3份,在120rpm的搅拌速率下 混炼15min,得中间反应产物;
(7)将步骤(6)的中间反应产物在150℃的条件下硫化45min,冷却至室温后得硫化反应物;
(8)将步骤(7)得到的硫化反应物粉碎成颗粒状,与丙烯酸异辛酯2份进行充分机械混匀并得到混合物料,随后将上述混合物料放置在预制的成型模具内进行热压,热压温度为100℃,热压时间为4h,热压完成后冷却至室温,得到成品材料。
实施例2
(1)将石英沙23份、高岭土17份、滑石粉10份混合均匀置于球磨机中,经湿法球磨,得到粒度170目的混合料浆;
(2)将羧基聚酯树脂25份置于反应釜中,升温至150℃,在真空度为-0.08Mpa的条件下处理2.5h,随后升温至175℃,加入四丁酚醛8份、聚己二酸乙二醇酯4份、甲氧基聚乙二醇3份,在常压下反应1h,将反应产物用3mol/L的稀盐酸洗涤2-3次,然后用去离子水洗涤至中性,得改性羧基聚酯树脂;
(3)将乙酰柠檬酸三丁酯11份、六次甲基四胺6份、磷酸钡2份混合,加入2000mL去离子水,进行超声处理,超声处理的条件为:温度55℃,超声功率800W,超声时间30min;得超声处理混合物;
(4)将步骤(1)得到的混合料浆干燥成粉,随后加入煅烧炉中,在1100℃下,煅烧50min,然后迅速降温至室温,得煅烧产物;
(5)将步骤(4)的煅烧产物加入反应釜中,加热反应釜,待温度达到115℃时,再向反应釜中加入步骤(2)所得的改性羧基聚酯树脂和步骤(3)所得的超声处理混合物,混合均匀后保温反应30min,得初步反应产 物;
(6)将步骤(5)所得的初步反应产物倒入混炼机中,调节混炼机温度至140℃,随后向混炼机中加入氯化石蜡4份,在135rpm的搅拌速率下混炼17min,得中间反应产物;
(7)将步骤(6)的中间反应产物在150℃的条件下硫化45min,冷却至室温后得硫化反应物;
(8)将步骤(7)得到的硫化反应物粉碎成颗粒状,与甘油二甲基丙烯酸酯3份进行充分机械混匀并得到混合物料,随后将上述混合物料放置在预制的成型模具内进行热压,热压温度为110℃,热压时间为4.5h,热压完成后冷却至室温,得到成品材料。
实施例3
(1)将石英沙25份、高岭土20份、滑石粉12份混合均匀置于球磨机中,经湿法球磨,得到粒度180目的混合料浆;
(2)将羧基聚酯树脂28份置于反应釜中,升温至150℃,在真空度为-0.08Mpa的条件下处理3h,随后升温至175℃,加入四丁酚醛10份、聚己二酸乙二醇酯5份、甲氧基聚乙二醇4份,在常压下反应1h,将反应产物用3mol/L的稀盐酸洗涤2-3次,然后用去离子水洗涤至中性,得改性羧基聚酯树脂;
(3)将乙酰柠檬酸三丁酯15份、六次甲基四胺9份、磷酸钡3份混合,加入2000mL去离子水,进行超声处理,超声处理的条件为:温度60℃,超声功率800W,超声时间35min;得超声处理混合物;
(4)将步骤(1)得到的混合料浆干燥成粉,随后加入煅烧炉中,在1200℃下,煅烧50min,然后迅速降温至室温,得煅烧产物;
(5)将步骤(4)的煅烧产物加入反应釜中,加热反应釜,待温度达到115℃时,再向反应釜中加入步骤(2)所得的改性羧基聚酯树脂和步骤(3)所得的超声处理混合物,混合均匀后保温反应30min,得初步反应产物;
(6)将步骤(5)所得的初步反应产物倒入混炼机中,调节混炼机温度至150℃,随后向混炼机中加入氯化石蜡5份,在150rpm的搅拌速率下混炼20min,得中间反应产物;
(7)将步骤(6)的中间反应产物在150℃的条件下硫化45min,冷却至室温后得硫化反应物;
(8)将步骤(7)得到的硫化反应物粉碎成颗粒状,与三乙醇胺4份进行充分机械混匀并得到混合物料,随后将上述混合物料放置在预制的成型模具内进行热压,热压温度为120℃,热压时间为5h,热压完成后冷却至室温,得到成品材料。
对比例1
(1)将石英沙30份、高岭土12份、滑石粉5份混合均匀置于球磨机中,经湿法球磨,得到粒度150目的混合料浆;
(2)将羧基聚酯树脂22份置于反应釜中,升温至150℃,在真空度为-0.08Mpa的条件下处理2h,随后升温至175℃,加入四丁酚醛6份、聚己二酸乙二醇酯3份、甲氧基聚乙二醇2份,在常压下反应1h,将反应产物用3mol/L的稀盐酸洗涤2-3次,然后用去离子水洗涤至中性,得改性羧基聚酯树脂;
(3)将乙酰柠檬酸三丁酯20份、六次甲基四胺12份、磷酸钡5份混合,加入2000mL去离子水,进行超声处理,超声处理的条件为:温度50 ℃,超声功率800W,超声时间25min;得超声处理混合物;
(4)将步骤(1)得到的混合料浆干燥成粉,随后加入煅烧炉中,在800℃下,煅烧50min,然后迅速降温至室温,得煅烧产物;
(5)将步骤(4)的煅烧产物加入反应釜中,加热反应釜,待温度达到115℃时,再向反应釜中加入步骤(2)所得的改性羧基聚酯树脂和步骤(3)所得的超声处理混合物,混合均匀后保温反应30min,得初步反应产物;
(6)将步骤(5)所得的初步反应产物倒入混炼机中,调节混炼机温度至120℃,随后向混炼机中加入氯化石蜡2份,在120rpm的搅拌速率下混炼15min,得中间反应产物;
(7)将步骤(6)的中间反应产物在180℃的条件下硫化45min,冷却至室温后得硫化反应物;
(8)将步骤(7)得到的硫化反应物粉碎成颗粒状,与丙烯酸异辛酯2份进行充分机械混匀并得到混合物料,随后将上述混合物料放置在预制的成型模具内进行热压,热压温度为100℃,热压时间为4h,热压完成后冷却至室温,得到成品材料。
对比例2
(1)将石英沙23份、高岭土17份、滑石粉10份混合均匀置于球磨机中,经湿法球磨,得到粒度170目的混合料浆;
(2)将乙酰柠檬酸三丁酯11份、六次甲基四胺6份、磷酸钡2份混合,加入2000mL去离子水,进行超声处理,超声处理的条件为:温度55℃,超声功率800W,超声时间30min;得超声处理混合物;
(3)将步骤(1)得到的混合料浆干燥成粉,随后加入煅烧炉中,在 1100℃下,煅烧50min,然后迅速降温至室温,得煅烧产物;
(4)将步骤(3)的煅烧产物加入反应釜中,加热反应釜,待温度达到115℃时,再向反应釜中加入羧基聚酯树脂25份和步骤(2)所得的超声处理混合物,混合均匀后保温反应30min,得初步反应产物;
(5)将步骤(4)所得的初步反应产物倒入混炼机中,调节混炼机温度至140℃,随后向混炼机中加入氯化石蜡4份,在135rpm的搅拌速率下混炼17min,得中间反应产物;
(6)将步骤(5)的中间反应产物在150℃的条件下硫化45min,冷却至室温后得硫化反应物;
(7)将步骤(6)得到的硫化反应物粉碎成颗粒状,与甘油二甲基丙烯酸酯3份进行充分机械混匀并得到混合物料,随后将上述混合物料放置在预制的成型模具内进行热压,热压温度为110℃,热压时间为4.5h,热压完成后冷却至室温,得到成品材料。
对比例3
(1)将石英沙25份、高岭土20份、滑石粉12份混合均匀置于球磨机中,经湿法球磨,得到粒度180目的混合料浆;
(2)将羧基聚酯树脂28份置于反应釜中,升温至150℃,在真空度为-0.08Mpa的条件下处理3h,随后升温至175℃,加入四丁酚醛10份、聚己二酸乙二醇酯5份、甲氧基聚乙二醇4份,在常压下反应1h,将反应产物用3mol/L的稀盐酸洗涤2-3次,然后用去离子水洗涤至中性,得改性羧基聚酯树脂;
(3)将乙酰柠檬酸三丁酯15份、六次甲基四胺9份、磷酸钡3份混合,加入2000mL去离子水,进行超声处理,超声处理的条件为:温度60 ℃,超声功率800W,超声时间35min;得超声处理混合物;
(4)将步骤(1)得到的混合料浆干燥成粉,随后加入煅烧炉中,在1200℃下,煅烧50min,然后迅速降温至室温,得煅烧产物;
(5)将步骤(4)的煅烧产物加入反应釜中,加热反应釜,待温度达到115℃时,再向反应釜中加入步骤(2)所得的改性羧基聚酯树脂和步骤(3)所得的超声处理混合物,混合均匀后保温反应30min,得初步反应产物;
(6)将步骤(5)的初步反应产物在150℃的条件下硫化45min,冷却至室温后得硫化反应物;
(7)将步骤(6)得到的硫化反应物粉碎成颗粒状,与三乙醇胺4份进行充分机械混匀并得到混合物料,随后将上述混合物料放置在预制的成型模具内进行热压,热压温度为120℃,热压时间为5h,热压完成后冷却至室温,得到成品材料。
将实施例1-3和对比例1-3的制得的建筑材料分别进行燃烧性能等级、抗渗等级、线性收缩率这三项测试,测试结果如表1所示。
表1
  燃烧性能 抗渗等级 线性收缩率(%)
实施例1 A级 P10 0.18
实施例2 A级 P10 0.15
实施例3 A级 P10 0.20
对比例1 A级 P8 0.86
对比例2 B1级 P6 1.33
对比例3 B1级 P8 0.92
本发明的用于外墙保温层的建筑材料制备方法通过将石英沙、高岭土、 滑石粉湿法球磨,干燥成粉后煅烧,再加入经改性的羧基聚酯树脂以及经超声处理的乙酰柠檬酸三丁酯、六次甲基四胺和磷酸钡的混合物共同进行加热反应,随后经混炼、硫化、热压等一系列特定工艺制成成品建筑材料。制备而成的建筑材料,其阻燃效果好,耐候、耐老化,具有较好的应用前景。本发明的用于外墙保温层的建筑材料的制备方法所用原料廉价、方法简单,适于大规模工业化运用,实用性强。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。

Claims (5)

  1. 用于外墙保温层的建筑材料制备方法,其特征在于,由以下步骤组成:
    (1)将石英沙20-25份、高岭土15-20份、滑石粉8-12份混合均匀置于球磨机中,经湿法球磨,得到粒度150-180目的混合料浆;
    (2)将羧基聚酯树脂22-28份置于反应釜中,升温至150℃,在真空条件下处理2-3h,随后升温至175℃,加入四丁酚醛6-10份、聚己二酸乙二醇酯3-5份、甲氧基聚乙二醇2-4份,在常压下反应1h,将反应产物用3mol/L的稀盐酸洗涤2-3次,然后用去离子水洗涤至中性,得改性羧基聚酯树脂;
    (3)将乙酰柠檬酸三丁酯6-15份、六次甲基四胺3-9份、磷酸钡1-3份混合,加入2000mL去离子水,进行超声处理,超声处理的条件为:温度50-60℃,超声功率800W,超声时间25-35min;得超声处理混合物;
    (4)将步骤(1)得到的混合料浆干燥成粉,随后加入煅烧炉中,在1000-1200℃下,煅烧50min,然后迅速降温至室温,得煅烧产物;
    (5)将步骤(4)的煅烧产物加入反应釜中,加热反应釜,待温度达到115℃时,再向反应釜中加入步骤(2)所得的改性羧基聚酯树脂和步骤(3)所得的超声处理混合物,混合均匀后保温反应30min,得初步反应产物;
    (6)将步骤(5)所得的初步反应产物倒入混炼机中,调节混炼机温度至130-150℃,随后向混炼机中加入氯化石蜡3-5份,在120-150rpm的搅拌速率下混炼15-20min,得中间反应产物;
    (7)将步骤(6)的中间反应产物在150℃的条件下硫化45min,冷却至室温后得硫化反应物;
    (8)将步骤(7)得到的硫化反应物粉碎成颗粒状,与交联剂2-4份 进行充分机械混匀并得到混合物料,随后将上述混合物料放置在预制的成型模具内进行热压,热压温度为100-120℃,热压时间为4-5h,热压完成后冷却至室温,得到成品材料。
  2. 根据权利要求1所述的用于外墙保温层的建筑材料制备方法,其特征在于,所述步骤(1)中球磨机的球料比为15:1。
  3. 根据权利要求1所述的用于外墙保温层的建筑材料制备方法,其特征在于,所述步骤(2)中的真空度优选为-0.08Mpa。
  4. 根据权利要求1所述的用于外墙保温层的建筑材料制备方法,其特征在于,所述步骤(8)中的交联剂选自丙烯酸异辛酯、甘油二甲基丙烯酸酯、三乙醇胺中的任意一种。
  5. 根据权利要求1-4任一项所述制备方法得到的用于外墙保温层的建筑材料在建筑墙体材料中的应用。
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